ASTM D4768-11
(Test Method)Standard Test Method for Analysis of 2,6-Ditertiary-Butyl Para-Cresol and 2,6-Ditertiary-Butyl Phenol in Insulating Liquids by Gas Chromatography
Standard Test Method for Analysis of 2,6-Ditertiary-Butyl Para-Cresol and 2,6-Ditertiary-Butyl Phenol in Insulating Liquids by Gas Chromatography
SIGNIFICANCE AND USE
In new electrical insulating oil, this test method provides a quantitative measure of the amounts of 2,6-ditertiary-butyl para-cresol and 2,6-ditertiary-butyl phenol that have been added to the oil. In a used oil, the test measures the amount of these inhibitors remaining in the oil. This test method is suitable for manufacturing control, specification acceptance, and service evaluation.
This test method is used to separate, identify, and quantify the inhibitors with minimal interference and matrix effects.
This test method has also been used successfully to determine the inhibitor concentrations in other insulating liquids such as esters and high-temperature hydrocarbons.
SCOPE
1.1 This test method covers the determination by gas chromatography of 2,6-ditertiary-butyl para-cresol and 2,6-ditertiary-butyl phenol in new and used insulating liquids at concentrations up to 0.5 %. It includes the determination in Type I and II insulating mineral oils as specified in Specification D3487, but has also been used to measure these inhibitors in other insulating liquids, such as esters and high fire-point hydrocarbons.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D4768 − 11
Standard Test Method for
Analysis of 2,6-Ditertiary-Butyl Para-Cresol and 2,6-
Ditertiary-Butyl Phenol in Insulating Liquids by Gas
1
Chromatography
This standard is issued under the fixed designation D4768; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 4. Significance and Use
1.1 This test method covers the determination by gas 4.1 Innewelectricalinsulatingoil,thistestmethodprovides
chromatography of 2,6-ditertiary-butyl para-cresol and 2,6- a quantitative measure of the amounts of 2,6-ditertiary-butyl
ditertiary-butyl phenol in new and used insulating liquids at para-cresol and 2,6-ditertiary-butyl phenol that have been
concentrations up to 0.5 %. It includes the determination in added to the oil. In a used oil, the test measures the amount of
Type I and II insulating mineral oils as specified in Specifica- these inhibitors remaining in the oil. This test method is
tion D3487, but has also been used to measure these inhibitors suitable for manufacturing control, specification acceptance,
in other insulating liquids, such as esters and high fire-point and service evaluation.
hydrocarbons.
4.2 This test method is used to separate, identify, and
1.2 This standard does not purport to address all of the
quantify the inhibitors with minimal interference and matrix
safety concerns, if any, associated with its use. It is the
effects.
responsibility of the user of this standard to establish appro-
4.3 This test method has also been used successfully to
priate safety and health practices and determine the applica-
determine the inhibitor concentrations in other insulating
bility of regulatory limitations prior to use.
liquids such as esters and high-temperature hydrocarbons.
2. Referenced Documents
5. Apparatus
2
2.1 ASTM Standards:
5.1 Gas Chromatograph, equipped with oven temperature
D923 Practices for Sampling Electrical Insulating Liquids
control constant to 1°C and with heated injector port.
D3487 Specification for Mineral Insulating Oil Used in
5.1.1 Means to Record the Chromatogram, such as a pen
Electrical Apparatus
recorder or a digital integrator to determine peak areas, is
D5222 Specification for High Fire-Point Mineral Electrical
recommended. An automated sample injector may be used.
Insulating Oils
E260 Practice for Packed Column Gas Chromatography
5.2 Flame Ionization Detector, with appropriate hydrogen/
air gas flows, is preferred over a thermal conductivity detector
3. Summary of Test Method
to provide maximum sensitivity.
3.1 The test specimen is placed onto a column containing
5.3 Column, a suitable stainless steel or glass column
activated alumina and extracted to remove interfering sub-
packed with a nonpolar silicone on an appropriate support or
stances. The inhibitors are then eluted from the column with
equivalent capillary column.
suitable solvent and analyzed by gas chromatography. The
3 4
inhibitor type and quantity are determined by comparison of NOTE 1—A 3 % OV-1 on 100/120 Mesh Supelcoport, 1.83 m (6 ft)
long, 3.2 mm (0.125 in.) in outside diameter has been used successfully.
each component with a working standard tested under similar
4
A SPB-1 30 m by 0.53 mm 1µm film column has also been used
conditions.
successfully.
5.3.1 Condition columns in accordance with manufacturer’s
1
This test method is under the jurisdiction of ASTM Committee D27 on
Electrical Insulating Liquids and Gases and is the direct responsibility of Subcom- recommendations. Disconnect columns from detector prior to
mittee D27.03 on Analytical Tests.
conditioning and reconnect after conditioning.
Current edition approved Aug. 1, 2011. Published September 2011. Originally
approved in 1988 as D4768 – 88. Last previous edition approved in 2003 as 5.4 Precision Syringe, glass, 10.0 µL.
D4768 – 03. DOI: 10.1520/D4768-11.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Registered trademark of Ohio Valley Specialty Co.
4
the ASTM website. Registered trademark of Supelco, Inc.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D4768 − 11
5.5 Volumetric Glassware, appropriate for making dilutions. 7.3.1 Prepare a check standard containing 0.30 % (w/w)
DBP and 0.30 % (w/w) DBPC in methanol. Dilute 0.25 mL of
5.6 Pipets, Pasteur, disposable, 146 by 7.5 mm.
check standard to 5.0 mL with methan
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D4768–03 Designation:D4768–11
Standard Test Method for
Analysis of 2,6-Ditertiary-Butyl Para-Cresol and 2,6-
Ditertiary-Butyl Phenol in Insulating Liquids by Gas
1
Chromatography
This standard is issued under the fixed designation D4768; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 Thistestmethodcoversthedeterminationbygaschromatographyof2,6-ditertiary-butylpara-cresoland2,6-ditertiary-butyl
phenol in new and used insulating liquids at concentrations up to 0.5 %. It includes the determination in Type I and II insulating
mineral oils as specified in Specification D3487, but has also been used to measure these inhibitors in other insulating liquids, such
as esters and high fire-point hydrocarbons.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D923 Practices for Sampling Electrical Insulating Liquids
D3487 Specification for Mineral Insulating Oil Used in Electrical Apparatus
D5222 Specification for High Fire-Point Mineral Electrical Insulating Oils
E260 Practice for Packed Column Gas Chromatography
3. Summary of Test Method
3.1 The test specimen is placed onto a column containing activated alumina and extracted to remove interfering substances.The
inhibitors are then eluted from the column with suitable solvent and analyzed by gas chromatography. The inhibitor type and
quantity are determined by comparison of each component with a working standard tested under similar conditions.
4. Significance and Use
4.1 In new electrical insulating oil, this test method provides a quantitative measure of the amounts of 2,6-ditertiary-butyl
para-cresol and 2,6-ditertiary-butyl phenol that have been added to the oil. In a used oil, the test measures the amount of these
inhibitors remaining in the oil. This test method is suitable for manufacturing control, specification acceptance, and service
evaluation.
4.2 This test method is used to separate, identify, and quantify the inhibitors with minimal interference and matrix effects.
4.3 This test method has also been used successfully to determine the inhibitor concentrations in other insulating liquids such
as esters and high-temperature hydrocarbons.
5. Apparatus
5.1 Gas Chromatograph, equipped with oven temperature control constant to 1°C and with heated injector port.
5.1.1 Means to Record the Chromatogram, such as a pen recorder or a digital integrator to determine peak areas, is
recommended. An automated sample injector may be used.
5.2 Flame Ionization Detector, with appropriate hydrogen/air gas flows, is preferred over a thermal conductivity detector to
provide maximum sensitivity.
1
This test method is under the jurisdiction ofASTM Committee D27 on Electrical Insulating Liquids and Gases and is the direct responsibility of Subcommittee D27.03
on Analytical Tests.
Current edition approved March 10, 2003. Published May 2003. Originally approved in 1988 as D4768–88. Last previous edition approved in 1996 as D4768–96. DOI:
10.1520/D4768-03.
Current edition approved Aug. 1, 2011. Published September 2011. Originally approved in 1988 as D4768 – 88. Last previous edition approved in 2003 as D4768 – 03.
DOI: 10.1520/D4768-11.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4768–11
5.3 Column, a suitable stainless steel or glass column packed with a nonpolar silicone on an appropriate support or equivalent
capillary column.
3 4
NOTE 1—A 3 % OV-1 on 100/120 Mesh Supelcoport, 1.83 m (6 ft) long, 3.2 mm (0.125 in.) in outside diameter has been used successfully. 1.83
4
m (6 ft) long, 3.2 mm (0.125 in.) in outside diameter has been used successfully. A SPB-1 30 m by 0.53 mm 1µm film column has also been used
successfully.
5.3.1 Condition
...
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